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  • Asaoka Et Al. (1978) - Observation of Hydrogen Trapping in Fe-0.15 WT% Ti Alloy by High Resolution Autoradiography

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    Observation of Hydrogen Trapping in Fe-0.15 Wt% Ti Alloy by High Resolution Autoradiography

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    Asaoka Et Al. (1978) - Observation of Hydrogen Trapping in Fe-0.15 Wt% Ti Alloy by High Resolution Autoradiography

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    Observation of Hydrogen Trapping in Fe-0.15 Wt% Ti Alloy by High Resolution Autoradiography

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    Asaoka Et Al. (1978) - Observation of Hydrogen Trapping in Fe-0.15 WT% Ti Alloy by High Resolution Autoradiography

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    PeterJonas
    Observation of Hydrogen Trapping in Fe-0.15 Wt% Ti Alloy by High Resolution Autoradiography

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    Observation of Hydrogen Trapping in Fe-0.15 Wt% Ti Alloy by High Resolution Autoradiography” T. ASAOKA, G. LAPASSET,") M, AUCOUTURIER, and P, LACOMBE* Abstract ‘The technique of microautoradiography at the electron microscope scale is used to describe the local repartition of hydrogen introduced by cathodic charging in an Fe-Ti alloy (0.15 Wt% Ti). The role of previous heat treatments of the alloy is studied. Different kinds of trapping sites for hydrogen are ‘observed, mainly decorated dislocations, grain boundaries and interfaces between TiC precipi tes and the matrix. A qualitative measurement of the quantity of trapped hydrogen and of the degassing rate leads to a classi tion of the taps with respect to their interaction energy with hydrogen, The consequence of carbonhydrogen interactions on the further cracking sensitivity of the all NY. influenced by the thermal history and carbide repartition, is discussed, ‘There have be steels because of the engines high strength steels, and recently for the austenitic stainless stools. However, the behavior of hydrogen obtained from varied environments and presont in supersaturated form in the material ‘and the mechanisms of embrittlement by this hydrogen are still being discussed. In a very simplified manner, one can say, from the most recent data, that, for low hydrogen fugacities, 2 mechanism based on lattice decohesion! is responsible for the embrittlement, while, for high fugacities, during the introduction of hydrogen, a pressure mechanism may operate.? In the case of cathodic charging, usually used in laboratory studies, hydrogen fugacity is at a very high level. To clarity where this supersaturated hydrogen segregates in the material or, in other words, at which sites this hydrogen is trapped, is of essential importance for the discussion of hydrogen embrittlement. ‘The principal aim of this study is to report direct observations ff hydrogen rapping by high resolution autoradiography and to give some information on the subsequent hydragen embrittlement, ina Fe-0.15 Wr% Ti alloy under cathodic charging conditions. many studies on the hydrogen embrittlement of ing importance, particularly for the Experimental Method Fe.0.15 We% Ti alloy was chosen to observe the trapping sites fof hydrogen in a simple structure, The rale of Ti addition is to getter the metalioid solute atoms (C, N, and O) as precipitates.” Some detailed results on the Behavior of cracks intraduced by cathodic charging in the same material have been reported* and shall be compared with our observations. 2) ‘The interstitial quantities are as follows: © = 18 ppm, N ppm, and © = 40 ppm. The specimens were cut from the as-received ingot 10 a dimension of 10 x 15 x 3 mm, and after five different heat treatments, were charged cathodically and observed by autoradiography, The aim of these treatments is to vary the distribution of precipitates and metalloid solute atoms, which depending on the treatment, can remain in a nongettered form in the matrix, and to submitted for publication March, 1977. “Laboratoire de Metallurgio Physique (associé au CNRS N° 177), Université de Paris Sud, 91405 Orsay Cedex, France. (Now at ONERA, Chatillon sous Bagneux, France. @rhe material was kindly supplied by |. M. Bernstein, Carnegie. Mellon University, Pittsburgh, Pennsylvania, for the purpose of cooperative research observe the variation of hydrogen trapping according to such ‘As shown in Table 1, specimens were at first maintained at 1150 C for 7 days in an attempt to dissolve all the preexisting precipitates back into solid solution. Specimens were cooled from 1150 C at two different cooling rates to vary the degree of distribution of these precipitates or solute impurities between the ‘grain boundaries and the mateix (treatment for specimen D and E). For specimen F, annealing at 400 C was done immediately after to eliminate the precipitates from grain quenching. Furthermore, boundaries, another series of specimens was prepared by reerystallizing at 800 C, after 80% cold rolling the same material as treated in specimen F The grain size after each heat treatment is shown in Table 2. After electrolytic polishing of each heat treated specimen, cathodic charging without applied stress was carried out in a solution of 1N H2S03 with 9 high specific activity of tritium (1.5 Curie/ec) at oom temperature To observe the behavior of cracks and ta investigate a difference in the “depth” Uie., energy) of hydrogen trapping (as described later), two charging conditions were used, that is, acurrent density 30 mAem® with a charging time of 10 hours, and a current density (of 5 mA/em? with a charging time of 2 hours Outgassing after cathodic charging, at room temperature and Under ambient pressure for long times, was carried out in order 10 ‘observe and confirm the difference in the interaction energy with hydrogen or the “depth” of each trap. The periods of outgassing are as follows: first stage, 1 day; second stage, 15 days; third stage, 35 days; and fourth stage, over 100 days. Observation of carbon distribution between the grain boundaries and. the matrix, by high resolution autoradiography, charging with '*C was carried out. The technique of 'C charging is ‘described. in detail elsewnere.® Our charging conditions are os totlows: '4¢ charging from BaC%O3 at 1000 C, 90 minutes, in a swaled silica capsule “> quenching into water + homogenizing at 1000 C, 68 hours, > quenching into water ~* heat treatments of Table 1 High resolution autoradiography was carried out on tritium and *c charged specimens by the method developed in our laboratory. Each charged and outgossed specimen wos electrolytically polished, etched, and a chromium carbon film was evaporated on the surface ‘A monogranular film of liquid photographic nuclear emulsion Uiford La) was costed directly on this evaporated film, and the (0010:9312/78/000001/83.00/0 Vol. 34, No. 2, February, 1978 ©1978, National Association of Corrosion Engineers 39 TABLE 1 — Heat Treatments of Specimens ‘Specimen Hat Treatment ° 1180 6, 168 hours> quench to -60 6 E 1150 6, 168 hours> furnace coo! (125 C/hours) 1180 6, 168 hours> quench to -60.C—ranneal at 400 C, 2hours a Specimen F -* 80% col roll “F800 C, 48 hours reerystallize ~ quench to -60.C 42 Specimen F -> 80% cold roll 800 C, 48 hours recrystallize > furnace cool TABLE 2 — Intergranular Cracking Aspects and Grain Size of Each Specimen ay Crack Froqueney| ‘Mean Crack Length ‘Moan Grain Size Specimen (%) (um) (um) > 3.0 150 260 e 13 290 560 F 24 120 260 HI 218 220 110 #2. 30 110 110 FIGURE 1 — Example of intergranular cracking (specimen oD. specimens were stored in a dark box under argon atmosphere at 30 c Exposure time was 6 to 20 days [depending on the activity of ‘each specimen) under these conditions, and they were developed by 1019 developer. After chemical stripping, observations were carried out on this replica-emulsion composite by 100 KV electron microscopy. Results Cracking Behavior Specimens charged cathodically in tritium + 1N H2S0g solution with high current density (30 mA/em?) and for a long time (10 hours) show considerable intergranular cracking, Table 2 indicates the cracking behavior as a function of heat treatments. In all cases, transgranular eracking was occasional found, but it was negligible compared with the intergranular cracking (Figure 1) ‘The cracking behavior of specimens D, E, and F cooled from 110 C at various cooling rates is different from that of specimens Hi and H2, recrystallized at 800 C. In the series HI and H2, the crack frequency is much higher than that of series O, &, and F, and taking into account the mean 40 grain size of each specimen, the mean crack length of H1 and H2 is longer and cracks extend over 2 or 3 grain boundaries, while in the series D, E, and F, the mean crack length is shorter than the mean grain boundary length. In each series, slight differences were found between D, F, and , as well as botwoen H1 and H2, Thus, the behavior of intergranular cracking caused by cathodic charging in these materials is greatly dominated by the heot treatment, i.e, the distribution of impurity atoms or the mor- phology of precipitates. So, at first, microstructures obtained by these five heat treatments were examined by electron microscopy and '*C auto- radiography. ‘Structures and '*C Autoradiography Precipitates in specimen F tempered at 400 © mostly form a continuous alignment along the grain boundaries (Figure 2a), while in specimen , grain boundary precipitates are less than in specimen F, but small precipitates are found on the polygonization network Which seems to be formed by the slow cooling from 1150 C, Grain boundary precipitates are found even in specimen O (quenched from 1150 C), but their frequency is much smaller than for specimen F. Sometimes in the matrix, groups of plate like and needle like precipitates can be observed (Figure 3a and Figure 4b). In specimens Ht and H2, which were prepared in order to romove the precipitates from the grain boundaries, many alignments of fine precipitate generated by breaking the grain boundary precipitates, are observed in the matrix. Grain boundaries are leaner, and also subgrain boundaries are clearly obterved (Figure 2b). To confirm these differences in distribution of precipitates and interstitial carbon atoms between the grain boundaries and the matrix, observations by autoradiography were carried out for each heat treated specimen after !*C charging In specimen © (quenched), the few grain boundary precipitates are labeled by silver grains of the autoradiography. Continuous segregation of carbon is observed (Figure 3a). When such segregation ‘exists, it is strongly labeled on the autoradiography with no ‘evidence of an underlying continuous precipitate and with a strong dependence on the grain boundary orientation. The ratio of labeled to nonlabeled grain boundaries can be roughly estimated a¢ 1:1 All the spherical precipitates are strongly labeled, but there are many plate like and needle like precipitates which are not labeled, and this may indicate @ difference in the structure of these precipitates. CORROSION-NACE b FIGURE 2 — Microstructures of heat treated spi indicating a difference in grain boundary precipitates (trans ‘mission electron microscopy). (a) Specimen F, and (b) specimen H1. Grain boundary labeling in specimen F is stronger than D, and ‘more continuous precipitation is observed (Figure 3b). The ratio of strongly labeled to weakly or nonlabeled boundaries is about 4:1 In specimen E, observed grain boundaries are few because of the large grain size. Most of the boundaries are laboled discontinuously Particularly in this type of specimen, the polygonization network is Clearly labeled. This labeling is not continuous but punctuated Al the spherical precipitates in the matrix are labeled in all the specimens. Although it is not likely that the filaments of silver individually dispersed in the matrix represent the existence of interstitial solute carbon atoms, it should be noted that the dispersed quantity seems larger in D and E than in F. (On the contrary, in the series of Ht and H2, there are not many precipitates on the boundaries (less than for specimen D), and so the boundary labeling is rare (Figure 3c). {In summary, from observations of thin foils, contiemed by '*c autoradiography, three types of carbon segregation could be observed: (1) large carbide precipitates in the grain boundaries (E and F) and in the matrix (D, E, F, H1 and H2), are observed as a discontinuous labeling by silver grains; (2) fine precipitation and/or solute carbon segregation in the grain boundaries (D, Ht and H2) observed as a continuous or weak discontinuous labeling of the boundaries; and (2) precipitation and/or solute carbon segregation fn dislocations (mostly E. Autoradiography with Tritium Autoradiography of specimens charged eathodically in tritium from IN HS0s solution indicated some peculiar aspects corre sponding with the variation of microstructures discussed, When specimens are charged by high current density (30 Vol, 34, No. 2, February, 1978 FIGURE 3 — Observation of grain boundary carbon seprega tion by '*C autoradiography on replica. (a) Specimen D, (b) specimen F, and (c) specimen H1. ‘mA/em?, 10 hours) which causes intergranular cracking, almost all the sites|which tend to trap hydrogen atoms are probably labeled with silver grains. But above all, throughout these five specimens, strong hydrogen segregations at the precipitate matrix interfaces are remarkably observed (Figures 4a, f), and itis followed in order by: {egregntions at grain boundaries, dislacation boundaries (Figure 4b, }, and dislocations (Figure 4d) ‘This labeling of precipitatematrix interfaces is different in aspect depending on the shape of the precipitates (needle, plate, a FIGURE 4 — Observed trap sites after strong cathodic charging. (°H autoradiography on replica (a) Close labeling of spherical precipitate (specimen OD), (b) labeling on the polygonization network (speci ), (e) labeling of subgrain boundary (specimen H1), from grain boundary (specimen E), (0) discrete laboling of needle like precipitate (spe labeling of small spherical precipitate alignment (specimen 2). sphere): around or on the spherical precipitates there is a closed and dense silver grain accumulation, and around the needle or plate ike precipitates a discrete labeling is observed when it exists (Figure 4e, Grain boundaries are labeled continuously in the D, E, and F series (Figure 5a, b), while in the series of H1 and H2, the silver ‘rain accumulations are more thick but more discrete (Figure Se). 42 It is always found that there is an apparent difference in the amount of silver grains depending on the crientation of each boundary {in the same specimen} as was found by autoradiography with 'e, When the spacimens are charged by low current density 1S mAlem?, 2 hours), cracks are not observed: the labeling by silver CORROSION-NACE FIGURE 5 — Difference in labeling of grain boundary after strong cathodic charging. (a) Specimen D, (b) specimen F, {and (¢} specimen Hi. gains at the grain boundaries in D, E, and F series is obsorved only {round the boundary precipitates (Figure 6a) In HI and H2 series charged under the same conditions, a woak labeling at boundaries is observed (Figure Gb). Interfaces of spherical procipitatematrix are strongly. and constantly labeled forall five specimens, but interfaces of needle or plate like procipitates are rarely labeled. Vol. 34, No. 2, February, 1978 2um a FIGURE 6 ~ Difference in labeling of grain boundary after ‘weak cathodic charging. (a) Specimen F, and (b) specimen rs The segragations on the polygonization network and dislocation lines have almost disappeared. |v summary, four kinds of hydrogen traps were observed by autoradiography: (1) procipitate-matei interfaces intergranular oF bulk precipitates) strongly labeled in all cases, forall specimens; (2), ‘grain boundary continuous labeling, observed in specimens D, E, ‘and F only for high charging current density, and in specimens HT ‘and 2, for all current densities; (3) dislocation segregations, observed only for high charging current density; and (4) plate like and needle like precipitatematrix interfaces, searcely and dis continuously labeled Outgassing of Trapped Hydrogen (Table 3) ‘As mentioned above, itis clear that a difference in the depth of ‘wap exists among several trap sites, nd in particular, the difference: in precipitate matrix interfaces and grain boundaries is obvious. To Confirm this fact, the outgassing behavior of each specimen at room temperature was studied. In D, E, and F series which were charged at 30 mAlem?, all the trap site labelings remain after 18 days outgassing (up 10 the second stage defined previously). Hawever, after 35 days outgassing (the thied stage), continuous labeling of grain boundaries in specimen D and E becomes very weak oF nearly disappears. In specimen F, only residual weak silver grain clusters are observed at some boundaries, but the outgassing rate is much less than for specimens D and € ‘After outgassing 100 days (the fourth stage), grain boundary trapping in D and E have almost disappeared, and so the boundary labeling in F decreases too (Figure 7a), 43 TABLE 3 ~ General Aspect of Labeling (After Strong Cathodic Charging of ?H) Stage of Ongena teste 2nd Ste 2rd Stage 49 stage Proc Prin Prin. Prelp. Mat, Disloc,,, Gran. -Matsix isle. Genin Matrix ‘Oiloe, Grain Matric ioe, Trap Site tnter.) —poundary) Boundary Inter, Boundary Boundary ter Goundaryoundery Inert. Boundary Specimen ° m3 3 7 ome mm ma & ae m3 me mo mm mt mm mmm F m m3 moms m2 om m™ om Ht ms ™ ma m2 m3 mt mmm mmm He ms 3 m2 m2 ms mt mmm mmm ‘Notes mO™= ne abling, mt = very weak Ibeling, m2 = dr (DLavetng of pracistte on the grain boundries are not counted, 2 \vidnout the meet and pate ike provoiates OMinlades e sbgeain Boundaries In contrast with this, throughout all the specimens of D, E, and F series, the aspect of silver grain accumulations at precipitate interfaces does not change even after outgassing 100 days whether such precipitates exist in the matrix or at the boundary. The other types of labeling (dislocations, etc.) have almost disappeared after this third stage, apart from a few discrete silver gain accumulations on the polygonization network, probably ‘associated with fine precipitates In the strongly charged (30 mA/em?) HI and H2 specimens, after outgassing to the third stage, the silver grain accumulations ‘around the precipitates (in the matrix and at boundaries, become very weak or rarely observed, The outgassing rate seems faster than {or specimen F (Figure 7b, c). “The summary of these outgassing results is given in Table 3, Discussion Hydrogen Trapping “Morphological Aspect. It is generally considered that hydrogen concentrations in the cathodically charged materials can reach very high values {over 10* atm, and that supersaturated hydrogen in the lattice is mainly trapped by some lattice defects. Many studies on the diffusion coefficient of hydrogen in iron” show that, when diffusion coefficient is plotted against temperature, the activation energy is found to be 2 to 3 Keal/mol in the high Temperature range, and this is thought to correspond with a jump of hydrogen atom to adjacent interstitial site [At lower temperatures (near room temperature, this activation energy increases, and this suggests that the trapping-detrapping process isthe rate controlling mechanism for transport. Many defects are proposed to behave as trapping sites, for example: inclusions, mierovoids,” grain boundaries,” precipi tates,!"!? dislocations,! 9! interstitial atoms,"® vacancies, ete Due to the difference in aumber or quality of each trap, the behavior of hydrogen embrittlement will vary. Observations of tritium autoradiography in five kinds of specimens have shown three types of trapping: (1) trapping on precipitate-mstrix interfaces (in all cases); (2) trapping on grain boundaries; and (3) trapping on dislocation boundaries, especially ia specimens E, H1 and H2. ‘All these observations have been confirmed by transmission electron microscopy and thin foil microautoradiography. From the morphological aspect, one can differentiate between {11 strong labeling of the large precipitates in the matrix or the grain boundaries (with the exception of plate like and needle like precipitates); (2) @ week discrete labeling of some grain boundaries and dislocations; and (3) 2 continuous labeling of some grain boundaries ‘These morphological differences can be qualitatively attributed to the differences of trapping efficiency of the sites. This efficiency is 8 function of the wepping energy. The study on the role of variation of the charging current density and on outgassing behavior can quantify this hierarchy between trapping energies. Energetical Aspect. First, the energetic aspect of trapping is 44 Tabi, endl = song ond continuous labeling, observed with 2 change in charging current density and tong ‘outgassing at room temperature, It must be mentioned that all observations are made after @ prior outgassing of 20 hours at room temperature, This means that low energy traps (i.e, sites with low interaction with hydrogen), which outgss very rapidly, are never observed. Differences in charging current density are considered to influence the surface fugacity of hydrogen and, consequently, the filling efficiency of trapping sites. From our results, most of the trapping sites such 3s grain boundaries, precipitate-matrix interfaces, and dislocation boundaries {are labeled with strong charging condition of 30 mA/em?, 10 hours. On the contrary, with weak charging (5 mA/em?, 2 hours), the labeling on grain boundaries and dislocation boundaries decreases in D, E, and F series, and becomes very weak in H1 and H2 series, but strong precipitate-matrix interfacial labeting is stil observed, ‘The results of outgassing experiments (summarized in Table 3) confirm the following general hierarchy in the trapping energy of, the different sites: (1) precipitatematrix interface, (2) grain boundaries, and (3) other sites. ‘The extent of interaction between hydrogen and a trap site is considered to be represented by the gain of free enthalpy AGx between the normal lattice position and the position occupied by ‘rapped hydrogen,'° and an example of calculation of this AGx value for the most strong traps in maraging steel is obtained by photosnalysis of high resolution autoradiography.!® ‘According to this author, the inclusion-matrix interfaces ara the strongest trapping in this material, and a value of AGx?*° = -14.5 Keal/mol is obtained. This value, with the values of hydrogen fugacity and trap density which were calculated at the same time, is in good agreement, in magnitude, with the results of other enon tonsa In our case of Fe.0.15% Ti alloy, the large heterogeneity of hhydrogen localization due to the existence of many eracks in the specimen after witium charging, makes it difficult to calculate energies from the autoradiography observations, but it seems reasonable to propose a similar order of magnitude (> 14.5 Keal/mol) for the trapping energy. High temperature outgassing experiments, now in progress, will quantity this value more precisely. A goin in enthalpy for grain boundary trapping of 60,€>H2,H1 ” Role of Impurities and Structure on the Trap Site Property. Properties of the trap sites (particularly of grain boundaries and precipitate interfaces) are considered to be influenced by impurity ‘atoms and physical structure (eg, coherency of interface), and the Vol. 34, No. 2, February, 1978 ‘AGx value described above will thus vary. Impurity atoms seem to affect each trap (especially at the grain boundary) by combined interaction of some elements rather than individual effect of one element. In the following, the grain boundary and precipitate interface ate taken as typical trap sites and the influence of impurities and structure on each trip site is considered, Grain Boundary. As shown in the results of 'C auto radiography, the important behavior of carbon as an impurity atom is its partitioning between matrix and grain boundary with various heat teeatments Observed grain boundary segregation of carbon is more impor- tant when the cooling rate from solid solution treatment tempera- ture is slow; however, as described earlier, in many cases, there are precipitates at grain boundaries, Therefore, itis appropriate to say that the carbon is segregated in the form of carbides or around the carbides at grain boundaries rather than present in grain boundaries at solute atom sites. These differces in carbon partitioning are also shown by other authors,"*?° and will be closely related with the intergranular cracking. From our results of '*¢ autoradiography, the order of the extent of grain boundary segregation of carbon is as follows: F>ESD>H2>HI @ Bernstein and Rath?! proposed a model of interaction between Fe.C-H-0 at grain boundaries in decarburized iron and discussed a Probable explanation of intergranular cracking differences, which depends on the state of hydrogen: if carbon makes intergranular complexes with Fe and/or oxygen, hydrogen would be in an isolated solute state in the grain boundaries, while the absence of inter: ‘granular carbon segregation favors the formation of complexes Containing hydrogen, which would inhibit the brittleness. Our results seem to be contradictory with this model, In this model carbon atoms which constitute the complex are considered to be in the interstitial solute state. When carbon exists at grain boundaries inthe form of carbides, hydrogen segregates at the interfaces of such carbides, so in this case, two influences (interstitial complex and carbide) will be superimposed of these two influences, which has a major effect on the AGx value of grain boundary When the labeling of grain boundaries revealed by the auto: radiography is discrete, and this is the general case, it can be reasonably supposed that the trapping on carbide precipitates or on zones of high atomic porosity is predominant. The interstitial complex effects will appear only in specimens with no or few ‘intergranular carbide precipitations, in agreement with the propos: tions of Reference 21 (On the other hand, the role of other impurities which may interact with carbon andor hydrogen should be taken into ‘A-combination of the proposed hierarchy of WAG! values and carbon partition observations shows that the trapping energy is strongly ‘elated ro the nature of carbon segregation and/or precipitation: strong interaction with hydrogen of large carbides, ow interaction with hydrogen of segregated or finely precipitated carbon on grain boundaries and dislocations, and very weak interaction with grain boundaries free of carbon, even if the trapped ‘quantity i of the seme order of magnitude (specimens HT and H2). Tre intluence of structure of the grain boundaries on their ‘rapping ability is shown by the selectivity of autoradiographic labeling. Even in the specimens whieh reveal strong segregation of hydrogen at boundaries, the coexistence of fairly labeled boundaries and less labeled boundaries is observed. For example, as shown in Figure 7o, cases where two boundaries are well labeled and another is not labeled at the tripte point are often found. This heterogeneity is also found in '*C autoradiography labeling and can be attributed to the degree of misorientation atomic porosity or coherency) of ‘ach grain boundary. Misorientation of subgrain boundaries which are constituted by dislocations is very small in comparison with that of grain boundaries, and their coherency is considered to be stronger. ‘Tritium autoradiograph labeling of these dislocation boundaries is 45 very weak, except around carbides. Bernstein found a similar selectivity of intergranular cracking in cathodically hydrogen charged Fe-Ti alloy and drew the tame conclusion. Precipitate-Matrix Interface. As shown in the section on tritium autoradiography observation, the labeling aspect of precipi- ‘wtematrix interface is different, depending on the type of precipitate; strong trapping is observed on the spherical precipitates hich are considered to be titanium carbide (or carbo-nitride), and ‘weak trapping is found around the needle and plate like precipitates By electron diffraction, these needle and plate like precipitates, were determined to be FogN and TiN precipitates. ‘Such differences in interaction with hydrogen due to the ‘composition of precipitates are found in other Fe-C alloys between FeaC and Fe3C,"” and furthermore, there isthe other possibility of {an interaction of hydrogen and sulfide. ** ‘These differences are not only due to the chemical composition of the precipitates. It is also possible that the shape and size of precipitates controls the interaction of hydrogen with the interfaces. For example, in ferrite, spherical and lamellar carbide can play a different contribution to the interaction with hydrogen,?? and this shape and size effect is related to the coherency of interface, Here 0 apparent difference of trapping between the grain boundary ‘carbides and matrix carbides have been found. Intergranular Cracking ‘As described earlier, there is a strong difference in the cracking ‘behavior between D, E, and F series and H1 and H2 series, and in the latter case, the number of cracks observed at grain boundaries is large. ‘The grain size of specimen Hi and H2 is relatively smaller and the mean crack length is larger than D, E, and F, 9s found in Table 2 Generally, in pure iron and Fe-Ti alloy, decreasing the grain size decreases hydrogen induced cracking,?! and decreases the crack length.*® So the difference in cracking behavior between the two series of specimens in this work cannot be attributed to a grain size effect.® It should be noted too, that there is a difference in cracking percentage between H1 and H2, depending on the cooling rate after 800 C recrystallization, even if there is no difference in grain size. ‘Observed order of intergranular cracking tendency is as follows: E

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